负热膨胀材料立方ZrMo2O8的制备研究

以ZrO(NO3)2和N6H24Mo7O24·4H2O等为原料,采用湿化学法制备出立方相ZrMo2O8粉体.对前驱体在室温～800℃进行了TG-DSC测试,采用XRD、SEM对立方相ZrMo2O8粉体进行了分析观测.结果表明亚稳相立方ZrMo2O8的制备对热处理工艺十分敏感,采用湿化学法在450℃制各出单一立方相ZrMo2O8粉体,在室温～400℃热膨胀系数为-4.337×10-6K-1.     

Surface Pretreatments of Silicon Nitride for CVD Diamond Deposition

The efficiency of different surface pretreatments (four standard chemical etchings and four diamond powder abrasive procedures) on silicon nitride (Si₃N₄) substrates for chemical vapor deposition (CVD) of diamond has been systematically investigated. Blank Si₃N₄ samples were polished with colloidal silica (∼0.25 μm). Diamond nucleation and growth runs were conducted in a microwave plasma chemical vapor deposition apparatus for 10 min and 6 h, respectively. Superior results concerning nucleation density ( N _d∼ 10¹⁰ cm⁻² after 10 min), film uniformity, and grain size (below 2 μm after 6 h) were obtained for the mechanically microflawed samples, revealing that chemical etchings (hot and cold strong acids, molten base or CF₄ plasma) are not crucial for good CVD diamond quality on Si₃N₄.     

Nile blue adsorbed onto silica gel modified with niobium oxide for electrocatalytic oxidation of NADH

A study of modified carbon paste electrode employing Nile blue (NB) adsorbed on silica gel modified with niobium oxide (SN) for electrocatalytic oxidation of reduced nicotinamide adenine dinucleotide (NADH) is described. The adsorbed organic dye on SN was used to prepare a modified carbon paste electrode to investigate its electrochemical properties. The formal potential (E°′) of the adsorbed NB (−230 mV vs. saturated calomel electrode, SCE) showed a shift of 70 mV towards a more positive potential value, compared to NB dissolved in aqueous solution. In solutions with pH between 6.0 and 8.0 did stability and E°′ remained almost constant. However, for a solution pH lower than 6.0 the E°′ was affected by the acidity of the contacting solution, shifting the E°′ towards more positive values. For the solution pHs between 6.0 and 8.0 the electrocatalytic activity remained almost constant. A linear response range for NADH between 1.0×10⁻⁵ and 5.2×10⁻⁴ mol l⁻¹, at pH 7.0, was observed for the electrode, with an applied potential of −200 mV versus SCE. The formation of an intermediate charge transfer (CT) complex was proposed to the CT reaction between NADH and adsorbed NB. The heterogeneous electron transfer rate, k_obs, was 1400 M⁻¹ s⁻¹ and the apparent Michaelis-Menten constant, was 0.21 mM at pH 7.0 evaluated from rotating disk electrode (RDE) experiments with an electrode coverage of about 5.2×10⁻⁹ mol cm⁻². The increase in the reaction rate between NADH and the immobilized NB compared to those obtained with dissolved NB was assigned to the shift of the E°′ towards more positive values.     

Study of the polymerization of 1-octadecene with different rnetallocene catalysts

Summary 1-Octadecene (C18) was polymerized by using different metallocene catalysts. The rac-Et(Ind)₂ZrC1₂/MAO (I) and rac-Me₂Si(Ind)₂ZrC1₂/MAO (III) presented the highest activity as compared with ra-Et(2-Me-Ind)₂ZrCl₂/MAO (II) and Ph₂C(Flu)(Cp)ZrC1₂/MAO (IV) catalysts. Catalyst IV produced polymers with highest molecular weights. The microstructure of the polymers was determined by ¹³C-NMR spectroscopy. Catalyst systems I, II and III produced isotactic polymers while catalyst IV produced polymers with mainly syndiotactic structures but with large amount of stereoregular error. Received: 21 June 2002/Revised version: 4 November 2002/ Accepted: 4 November 2002     

Isobaric vapor—liquid equilibria for binary systems composed of methyl butanoate with ethanol and with propan-1-ol at 114.66 and 127.99 kpa

Vapor-liquid equilibrium data for the binary systems methyl butanoate/ethanol and methyl butanoate/propan-l-ol at pressures of 114.66 and 127.99 kPa are presented. Both mixtures yield an azeotrope, the compositions (ester) of which decrease quasi-linearly as the pressure increases. The experimental data for all the binary mixtures were fitted to a suitable equation and then used for comparison with predictions by ASOG and UNIFAC methods. These group contribution models give a good estimation of activity coefficients with an overall mean error less than 5% for all cases.     

含水量对渠道保温板保温耐久性的影响及保温板厚度设计

北方渠道大多使用保温板防止混凝土衬砌受冻胀破坏。在计算保温板厚度时为了降低成本,容易忽略保温板使用过程中受各种因素的影响导致保温效果变差的情况,使混凝土衬砌达不到设计使用年限便提前被破坏。内蒙古河套灌区试验结果表明,由于受酸雨、冻融作用、含水量等因素的影响,保温板保温效果平均每年降低0.9℃,其中受含水量变化的影响最大。经试验测得:聚苯乙烯保温板(EPS)含水量每增加1%,会导致导热系数增大5%。基于多层材料串联热阻叠加原理和热阻等效原理,对保温板厚度计算公式进行完善,并提出相应的铺设方法和施工技术要求。该设计对保温板在季节性冻土区的推广应用具有一定参考价值。     

非水溶剂回滴法测定低镍甲烷化催化剂的表面酸性

本文采用非水溶剂回滴法测定了低镍甲烷化催化剂和载体γ—Al2O3的表面酸性，并与催化剂的活性、组成、比表面积关联。实验结果说明，助剂的种类、含量对表面酸性有明显影响，催化剂催化活性与表面酸性关系不大。     

塑胶漆用的聚醚聚氨酯预聚物的研制

以TDT、TMP、N-220、3010、为主要原料合成聚醚型聚氨酯预聚物，达到塑胶漆的性能要求。本文探讨了不同的合成条件对预聚物的影响。     

用酰胺缩醛合成1,4,7,10-四氮杂十二烷的研究

用甲苯作溶剂,使三乙烯四胺和N,N-二甲基甲酰胺二甲基缩醛在85℃反应2h,得到中间体双咪唑啉,产率90.4%,在乙腈溶剂中,碳酸钾存在下,双咪唑啉和1,2-二溴乙烷进行扩环反应,得到环状中间体一溴盐,产率78.7%,一溴盐经碱性水解2h,得到1,4,7,10-四氮杂十二烷,产率74.2%。用元素分析、质谱和核磁共振氢谱对目标化合物进行了表征。     

Blends of polyamide 6 with bisphenol-A polycarbonate. I. Thermal properties and compatibility aspects

Blends of polyamide 6 (PA6) and polycarbonate (PC) have been investigated, over a full range of composition, to check interactions between them. SEM observations show that the mixtures are characterized by domains of clearly segregated homophases and voids between the two polymers. DSC and DMTA data indicate the presence of two T_g' s, corresponding to two separate phases, with the T_g of the PC phase decreasing on increasing the PA6 amount. Moreover, the crystallization kinetics of PA6 is slightly showed down by the PC. Chemical reactions between the two polymers are supposed to give rise to low molar mass compounds, as shown by GPC; these species plasticize the PC and partially dissolve into the molten polyamide, causing decrease of PC T_g and reduction of overall crystallization rate of PA6. Apparent influence of PC on melting temperature and enthalpy of PA6 is also discussed.